CN106803582A - A kind of anode material of lithium-ion battery and preparation method thereof - Google Patents
A kind of anode material of lithium-ion battery and preparation method thereof Download PDFInfo
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The invention belongs to sodium-ion battery preparing technical field, a kind of anode material of lithium-ion battery, including MIL 125 (Ti), sodium dihydrogen phosphate, ammonium dihydrogen phosphate and solvent are specifically disclosed.Its preparation method is：MIL 125 (Ti), sodium dihydrogen phosphate and ammonium dihydrogen phosphate are dissolved in a solvent respectively first, and is mixed, stirred, react to obtain mixed liquor, be evaporated the solvent in mixed liquor, obtain white solid powder；White solid powder is calcined in atmosphere furnace again, obtains black solid powder, obtained final product.Preparation method is simple of the invention is easy, and a step realizes NaTi2(PO4)3Compound with conductive carbon material, the anode material of lithium-ion battery specific capacity for preparing is higher, and cyclical stability is preferable.
Description
Technical field
The present invention relates to sodium-ion battery preparing technical field, and in particular to a kind of anode material of lithium-ion battery and its system
Preparation Method.
Background technology
With the progress and the development of society of science and technology, the energy and environmental problem have turned into the most important class in the world today
One of topic.Fossil fuel is still to use most energy in the world at present, but the reserves of fossil energy are limited, and the mankind are increasingly
Increased demand and be not added with restraining exploitation, inevitably result in the exhaustion of fossil energy.Therefore, new regenerative resource is found
And scale energy storage is extremely urgent.In many energy storage fields, electrochemical energy storage is a kind of simple and efficient energy storage mode.Its
In, lithium ion battery is the electrochemical power source being widely used at present, but as the industries such as number, traffic are relied on lithium ion battery
Aggravation, limited lithium resource will face shortage problem.Room temperature sodium-ion battery is widely distributed due to abundant raw material, and price is low
It is honest and clean, the extensive research interest of people is caused, its research and development can be relaxed to a certain extent because lithium resource shortage triggers
Battery development limitation problem.
Current anode material of lithium-ion battery mainly includes hard carbon, alloy and ti-based compound.Hard carbon is most widely used
One Na-like ions cell negative electrode material, but because sodium ion radius is larger, in the embedding/de- more difficult of graphite layers, and first
Irreversible SEI passivation layers are easily formed during discharge and recharge, causes first week coulombic efficiency reduction, this is the master for restricting such carbon material application
Want factor.There is serious volumetric expansion in metal simple-substance or alloy, cause capacity quickly to decline during sodium ion intercalation/deintercalation
Subtract, electrode stability reduction.Titanium-based oxide, as anode material of lithium-ion battery, is stored up by embedded category reaction mechanism
Sodium, however, due in itself crystal structure storage site it is limited, cause this kind of material storage sodium capacity generally relatively low.
NaTi2(PO4)3It is a kind of sodium ion electrode material, but because its electronic conductivity is relatively low, causes the electric discharge of material
Capacity is low, and high rate performance and cyclical stability are poor.
The content of the invention
For problems of the prior art, it is an object of the invention to provide a kind of anode material of lithium-ion battery and
Its preparation method, the method is simple and easy to apply, and the anode material of lithium-ion battery specific capacity of preparation is larger, preferable stable circulation
Property.
In order to achieve the above object, the present invention is achieved using following technical scheme.
(1) a kind of anode material of lithium-ion battery, it is characterised in that including following raw material components：MIL-125 (Ti), phosphorus
Acid dihydride sodium, ammonium dihydrogen phosphate and solvent.
Preferably, the solvent is methyl alcohol or absolute ethyl alcohol.
Preferably, in the raw material components, the mol ratio of MIL-125 (Ti), sodium dihydrogen phosphate and ammonium dihydrogen phosphate
It is (1:3:8)-(1:7:12).
(2) a kind of preparation method of anode material of lithium-ion battery, it is characterised in that comprise the following steps：
Step 1, MIL-125 (Ti), sodium dihydrogen phosphate and ammonium dihydrogen phosphate is dissolved in a solvent respectively, and mixed
Close, stir, react, obtain mixed liquor, be evaporated the solvent in the mixed liquor, obtain white solid powder；
Step 2, the white solid powder is calcined in atmosphere furnace, obtains black solid powder, is obtained final product.
Used as preferred, in step 1, the temperature of the reaction is 30-60 DEG C, and the time of the reaction is 20-28h.
Preferably, in step 2, the protective atmosphere in the atmosphere furnace is argon gas.
Preferably, in step 2, the temperature of the calcining is 500-900 DEG C, and the time of the calcining is 4-7h.
Preferably, in step 2, during the calcining, heating rate and rate of temperature fall be respectively 2-3 DEG C/
min。
Compared with prior art, beneficial effects of the present invention are：
The present invention with MOFs materials (MIL-125 (Ti)) as presoma, it is anti-with sodium dihydrogen phosphate, ammonium di-hydrogen phosphate
Should, on the one hand MIL-125 (Ti) can provide titanium source as presoma, on the other hand because the organic ligand of MOFs materials is lazy
Property atmosphere under calcine after can be changed into carbon, so as to prepare anode material of lithium-ion battery NaTi2(PO4)3/C.With other sodium
The preparation method of ion battery cathode material is compared, and preparation method is simple of the invention is easy, and a step realizes NaTi2(PO4)3
It is compound with conductive carbon material.Sodium-ion battery specific capacity prepared by preparation method of the invention is higher, cyclical stability and times
Rate excellent performance.
Brief description of the drawings
The present invention is described in further details with specific embodiment below in conjunction with the accompanying drawings.
Fig. 1 is the NaTi that embodiment 1 is obtained2(PO4)3The XRD of/C；In figure, abscissa is the incident angle of x-ray
Twice, unit is degree；Ordinate is intensity；
Fig. 2 is the NaTi that embodiment 1 is obtained2(PO4)3Charging and discharging curve figure of/C the electrodes under 20mA/g current densities；Figure
In, abscissa is specific capacity, and ordinate is voltage；Wherein, 1,5,10,20,30 cycle-index is represented in figure；
Fig. 3 is the NaTi that embodiment 1 is obtained2(PO4)3The cycle performance figure of/C electrodes；Abscissa is cycle-index, indulges and sits
It is designated as specific capacity.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
It will be appreciated that the following example is merely to illustrate the present invention, and it is not construed as limiting the scope of the present invention.
Embodiment 1
A kind of anode material of lithium-ion battery, expression formula is NaTi2(PO4)3/ C, prepares according to following steps：
Step 1, takes 0.036g MIL-125 (Ti), 0.012g sodium dihydrogen phosphates and 0.023g ammonium di-hydrogen phosphates and (rubs respectively
You are than being 1:5:10) it is dissolved separately in 20mL absolute ethyl alcohols, three kinds of solution is mixed, stirring reaction under the conditions of 40 DEG C of water-bath
After 24h, absolute ethyl alcohol is evaporated, obtain white solid powder.
Step 2,5h, the heating rate in calcination process are calcined for 700 DEG C by white solid powder in the atmosphere furnace of argon gas
3 DEG C/min is respectively with rate of temperature fall, black solid powder 0.23g is obtained.
Embodiment 2
A kind of anode material of lithium-ion battery NaTi2(PO4)3/ C, prepares according to following steps：
Step 1, takes 0.036g MIL-125 (Ti), 0.0096g sodium dihydrogen phosphates and 0.021g ammonium di-hydrogen phosphates and (rubs respectively
You are than being 1:4:9) it is dissolved separately in 20mL absolute ethyl alcohols, three kinds of solution is mixed, stirring reaction 24h under the conditions of 40 DEG C of water-bath
Afterwards, absolute ethyl alcohol is evaporated, white solid powder is obtained.
Step 2,5h, the heating rate in calcination process are calcined for 700 DEG C by white solid powder in the atmosphere furnace of argon gas
3 DEG C/min is respectively with rate of temperature fall, black solid powder 0.21g is obtained.
Embodiment 3
A kind of anode material of lithium-ion battery NaTi2(PO4)3/ C, prepares according to following steps：
Step 1, takes 0.036g MIL-125 (Ti), 0.014g sodium dihydrogen phosphates and 0.025g ammonium di-hydrogen phosphates and (rubs respectively
You are than being 1:6:11) it is dissolved separately in 20mL absolute ethyl alcohols, three kinds of solution is mixed, stirring reaction under the conditions of 30 DEG C of water-bath
After 24h, absolute ethyl alcohol is evaporated, obtain white solid powder.
Step 2,5h, the heating rate in calcination process are calcined for 700 DEG C by white solid powder in the atmosphere furnace of argon gas
3 DEG C/min is respectively with rate of temperature fall, black solid powder 0.24g is obtained.
Embodiment 4
A kind of anode material of lithium-ion battery NaTi2(PO4)3/ C, prepares according to following steps：
Step 1, takes 0.036g MIL-125 (Ti), 0.012g sodium dihydrogen phosphates and 0.023g ammonium di-hydrogen phosphates and (rubs respectively
You are than being 1:5:10) it is dissolved separately in 20mL absolute ethyl alcohols, three kinds of solution is mixed, stirring reaction under the conditions of 30 DEG C of water-bath
After 24h, absolute ethyl alcohol is evaporated, obtain white solid powder.
Step 2,5h, the heating rate in calcination process are calcined for 700 DEG C by white solid powder in the atmosphere furnace of argon gas
3 DEG C/min is respectively with rate of temperature fall, black solid powder 0.24g is obtained.
Embodiment 5
A kind of anode material of lithium-ion battery NaTi2(PO4)3/ C, prepares according to following steps：
Step 1, MIL-125 (Ti), sodium dihydrogen phosphate and ammonium di-hydrogen phosphate are taken respectively, and (mol ratio is 1:3:8) dissolve respectively
In 20mL absolute ethyl alcohols, three kinds of solution are mixed, under the conditions of 50 DEG C of water-bath after stirring reaction 24h, evaporate absolute ethyl alcohol, obtained
To white solid powder.
Step 2,5h, the heating rate in calcination process are calcined for 700 DEG C by white solid powder in the atmosphere furnace of argon gas
3 DEG C/min is respectively with rate of temperature fall, black solid powder 0.20g is obtained.
Embodiment 6
A kind of anode material of lithium-ion battery NaTi2(PO4)3/ C, prepares according to following steps：
Step 1, MIL-125 (Ti), sodium dihydrogen phosphate and ammonium di-hydrogen phosphate are taken respectively, and (mol ratio is 1:7:12) it is molten respectively
Solution mixes three kinds of solution in 20mL absolute ethyl alcohols, under the conditions of 60 DEG C of water-bath after stirring reaction 24h, evaporates absolute ethyl alcohol,
Obtain white solid powder.
Step 2,5h, the heating rate in calcination process are calcined for 700 DEG C by white solid powder in the atmosphere furnace of argon gas
3 DEG C/min is respectively with rate of temperature fall, black solid powder 0.23g is obtained.
Embodiment 7
A kind of anode material of lithium-ion battery NaTi2(PO4)3/ C, prepares according to following steps：
Step 1, takes 0.036g MIL-125 (Ti), 0.012g sodium dihydrogen phosphates and 0.023g ammonium di-hydrogen phosphates and (rubs respectively
You are than being 1:5:10) it is dissolved separately in 20mL absolute ethyl alcohols, three kinds of solution is mixed, stirring reaction under the conditions of 40 DEG C of water-bath
After 20h, absolute ethyl alcohol is evaporated, obtain white solid powder.
Step 2,5h, the heating rate in calcination process are calcined for 700 DEG C by white solid powder in the atmosphere furnace of argon gas
3 DEG C/min is respectively with rate of temperature fall, black solid powder 0.27g is obtained.
Embodiment 8
A kind of anode material of lithium-ion battery NaTi2(PO4)3/ C, prepares according to following steps：
Step 1, takes 0.036g MIL-125 (Ti), 0.012g sodium dihydrogen phosphates and 0.023g ammonium di-hydrogen phosphates and (rubs respectively
You are than being 1:5:10) it is dissolved separately in 20mL absolute ethyl alcohols, three kinds of solution is mixed, stirring reaction under the conditions of 40 DEG C of water-bath
After 26h, absolute ethyl alcohol is evaporated, obtain white solid powder.
Step 2,5h, the heating rate in calcination process are calcined for 700 DEG C by white solid powder in the atmosphere furnace of argon gas
3 DEG C/min is respectively with rate of temperature fall, black solid powder 0.25g is obtained.
Embodiment 9
A kind of anode material of lithium-ion battery NaTi2(PO4)3/ C, prepares according to following steps：
Step 1, takes 0.036g MIL-125 (Ti), 0.012g sodium dihydrogen phosphates and 0.023g ammonium di-hydrogen phosphates and (rubs respectively
You are than being 1:5:10) it is dissolved separately in 20mL absolute ethyl alcohols, three kinds of solution is mixed, stirring reaction under the conditions of 40 DEG C of water-bath
After 26h, absolute ethyl alcohol is evaporated, obtain white solid powder.
Step 2,5h, the heating rate in calcination process are calcined for 700 DEG C by white solid powder in the atmosphere furnace of argon gas
3 DEG C/min is respectively with rate of temperature fall, black solid powder 0.25g is obtained.
Embodiment 10
A kind of anode material of lithium-ion battery NaTi2(PO4)3/ C, prepares according to following steps：
Step 1, takes 0.036g MIL-125 (Ti), 0.012g sodium dihydrogen phosphates and 0.023g ammonium di-hydrogen phosphates and (rubs respectively
You are than being 1:5:10) it is dissolved separately in 20mL absolute ethyl alcohols, three kinds of solution is mixed, stirring reaction under the conditions of 40 DEG C of water-bath
After 28h, absolute ethyl alcohol is evaporated, obtain white solid powder.
Step 2,5h, the heating rate in calcination process are calcined for 700 DEG C by white solid powder in the atmosphere furnace of argon gas
3 DEG C/min is respectively with rate of temperature fall, black solid powder 0.19g is obtained.
Embodiment 11
A kind of anode material of lithium-ion battery NaTi2(PO4)3/ C, prepares according to following steps：
Step 1, takes 0.036g MIL-125 (Ti), 0.012g sodium dihydrogen phosphates and 0.023g ammonium di-hydrogen phosphates and (rubs respectively
You are than being 1:5:10) it is dissolved separately in 20mL absolute ethyl alcohols, three kinds of solution is mixed, stirring reaction under the conditions of 40 DEG C of water-bath
After 24h, absolute ethyl alcohol is evaporated, obtain white solid powder.
Step 2,5h, the heating rate in calcination process are calcined for 500 DEG C by white solid powder in the atmosphere furnace of argon gas
3 DEG C/min is respectively with rate of temperature fall, black solid powder 0.27g is obtained.
Embodiment 12
A kind of anode material of lithium-ion battery NaTi2(PO4)3/ C, prepares according to following steps：
Step 1, takes 0.036g MIL-125 (Ti), 0.012g sodium dihydrogen phosphates and 0.023g ammonium di-hydrogen phosphates and (rubs respectively
You are than being 1:5:10) it is dissolved separately in 20mL absolute ethyl alcohols, three kinds of solution is mixed, stirring reaction under the conditions of 40 DEG C of water-bath
After 24h, absolute ethyl alcohol is evaporated, obtain white solid powder.
Step 2,5h, the heating rate in calcination process are calcined for 600 DEG C by white solid powder in the atmosphere furnace of argon gas
3 DEG C/min is respectively with rate of temperature fall, black solid powder 0.27g is obtained.
Embodiment 13
A kind of anode material of lithium-ion battery NaTi2(PO4)3/ C, prepares according to following steps：
Step 1, takes 0.036g MIL-125 (Ti), 0.012g sodium dihydrogen phosphates and 0.023g ammonium di-hydrogen phosphates and (rubs respectively
You are than being 1:5:10) it is dissolved separately in 20mL absolute ethyl alcohols, three kinds of solution is mixed, stirring reaction under the conditions of 40 DEG C of water-bath
After 24h, absolute ethyl alcohol is evaporated, obtain white solid powder.
Step 2,5h, the heating rate in calcination process are calcined for 800 DEG C by white solid powder in the atmosphere furnace of argon gas
3 DEG C/min is respectively with rate of temperature fall, black solid powder 0.25g is obtained.
Embodiment 14
A kind of anode material of lithium-ion battery NaTi2(PO4)3/ C, prepares according to following steps：
Step 1, takes 0.036g MIL-125 (Ti), 0.012g sodium dihydrogen phosphates and 0.023g ammonium di-hydrogen phosphates and (rubs respectively
You are than being 1:5:10) it is dissolved separately in 20mL absolute ethyl alcohols, three kinds of solution is mixed, stirring reaction under the conditions of 40 DEG C of water-bath
After 24h, absolute ethyl alcohol is evaporated, obtain white solid powder.
Step 2,5h, the heating rate in calcination process are calcined for 900 DEG C by white solid powder in the atmosphere furnace of argon gas
3 DEG C/min is respectively with rate of temperature fall, black solid powder 0.27g is obtained.
Embodiment 15
A kind of anode material of lithium-ion battery NaTi2(PO4)3/ C, prepares according to following steps：
Step 1, takes 0.036g MIL-125 (Ti), 0.012g sodium dihydrogen phosphates and 0.023g ammonium di-hydrogen phosphates and (rubs respectively
You are than being 1:5:10) it is dissolved separately in 20mL methyl alcohol, three kinds of solution is mixed, under the conditions of 40 DEG C of water-bath after stirring reaction 24h,
Methyl alcohol is evaporated, white solid powder is obtained.
Step 2,4h, the heating rate in calcination process are calcined for 700 DEG C by white solid powder in the atmosphere furnace of argon gas
3 DEG C/min is respectively with rate of temperature fall, black solid powder 0.25g is obtained.
Embodiment 16
A kind of anode material of lithium-ion battery NaTi2(PO4)3/ C, prepares according to following steps：
Step 1, takes 0.036g MIL-125 (Ti), 0.012g sodium dihydrogen phosphates and 0.023g ammonium di-hydrogen phosphates and (rubs respectively
You are than being 1:5:10) it is dissolved separately in 20mL absolute ethyl alcohols, three kinds of solution is mixed, stirring reaction under the conditions of 40 DEG C of water-bath
After 24h, absolute ethyl alcohol is evaporated, obtain white solid powder.
Step 2,6h, the heating rate in calcination process are calcined for 700 DEG C by white solid powder in the atmosphere furnace of argon gas
3 DEG C/min is respectively with rate of temperature fall, black solid powder 0.24g is obtained.
Embodiment 17
A kind of anode material of lithium-ion battery NaTi2(PO4)3/ C, prepares according to following steps：
Step 1, takes 0.036g MIL-125 (Ti), 0.012g sodium dihydrogen phosphates and 0.023g ammonium di-hydrogen phosphates and (rubs respectively
You are than being 1:5:10) it is dissolved separately in 20mL absolute ethyl alcohols, three kinds of solution is mixed, stirring reaction under the conditions of 40 DEG C of water-bath
After 24h, absolute ethyl alcohol is evaporated, obtain white solid powder.
Step 2,7h, the heating rate in calcination process are calcined for 700 DEG C by white solid powder in the atmosphere furnace of argon gas
2 DEG C/min is respectively with rate of temperature fall, black solid powder 0.23g is obtained.
MIL-125 (Ti) in above-described embodiment 1-17 is terephthalic acids titanium salt, and its preparation method is：Take terephthalic acid (TPA)
0.5g, butyl titanate 0.26mL dry DMF in 10 milliliters with (volume ratio 9 in the mixed solution for drying methyl alcohol：1), indifferent gas
Hydro-thermal tank is transferred to after the lower stirring 30min of atmosphere protection and be put into temperature programmed control baking oven.It is raised to by room temperature with 3 DEG C/min temperature rates
150 DEG C and it is incubated 20h.White powder being obtained after cooling, a certain amount of methyl alcohol stirring 12h being taken and is displaced DMF, filtered, 100 DEG C are done
It is dry, obtain white powder, as MIL-125.
The anode material of lithium-ion battery NaTi prepared to embodiment 12(PO4)3/ C carries out XRD tests, as a result such as Fig. 1 institutes
Show.Diffraction maximum and NaTi in figure2(PO4)3Standard diagram diffraction maximum position consistency, shows to be made by the method for the present invention
Standby NaTi2(PO4)3Phase.
The anode material of lithium-ion battery NaTi prepared to embodiment 12(PO4)3/ C carries out electrochemical property test, as a result
As shown in Figures 2 and 3.As shown in Figure 2, there is NaTi in voltage 2.4v or so2(PO4)3Obvious charge and discharge platform, discharge and recharge
After the circle of circulation 30, specific discharge capacity is respectively 197,190mAh/g with charge specific capacity.
Additionally, the lithium ion battery negative material NaTi obtained by other embodiment2(PO4)3The chemical property of/C with it is upper
State conclusion basically identical.
Although the present invention is described in detail with a general description of the specific embodiments in this specification,
But on the basis of the present invention, it can be made some modifications or improvements, such as change the proportioning of reactant, change bath temperature, anti-
Between seasonable etc., this will be apparent to those skilled in the art.Therefore, without departing from theon the basis of the spirit of the present invention
These modifications or improvements, belong to the scope of protection of present invention.
Claims (8)
1. a kind of anode material of lithium-ion battery, it is characterised in that including following raw material components：MIL-125 (Ti), biphosphate
Sodium, ammonium dihydrogen phosphate and solvent.
2. anode material of lithium-ion battery according to claim 1, it is characterised in that the solvent is methyl alcohol or anhydrous second
Alcohol.
3. anode material of lithium-ion battery according to claim 1, it is characterised in that in the raw material components, MIL-125
(Ti), the mol ratio of sodium dihydrogen phosphate and ammonium dihydrogen phosphate is (1:3:8)-(1:7:12).
4. a kind of preparation method of anode material of lithium-ion battery, it is characterised in that comprise the following steps：
Step 1, MIL-125 (Ti), sodium dihydrogen phosphate and ammonium dihydrogen phosphate are dissolved in a solvent respectively, and are mixed, and are stirred
Mix uniform, reaction obtains mixed liquor, is evaporated the solvent in the mixed liquor, obtains white solid powder；
Step 2, the white solid powder is calcined in atmosphere furnace, obtains black solid powder, is obtained final product.
5. the preparation method of anode material of lithium-ion battery according to claim 4, it is characterised in that described in step 1
The temperature of reaction is 30-60 DEG C, and the time of the reaction is 20-28h.
6. the preparation method of anode material of lithium-ion battery according to claim 4, it is characterised in that described in step 2
Protective atmosphere in atmosphere furnace is argon gas.
7. the preparation method of anode material of lithium-ion battery according to claim 4, it is characterised in that described in step 2
The temperature of calcining is 500-900 DEG C, and the time of the calcining is 4-7h.
8. the preparation method of anode material of lithium-ion battery according to claim 7, it is characterised in that described in step 2
During calcining, heating rate and rate of temperature fall are respectively 2-3 DEG C/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108766772A (en) * | 2018-04-23 | 2018-11-06 | 华东师范大学 | A kind of carbon coating titanium phosphate sodium and its preparation and application |
| CN111525122A (en) * | 2020-05-12 | 2020-08-11 | 喻明兵 | NaTi2(PO4)3Negative electrode material of-porous carbon nanofiber sodium ion battery and preparation method thereof |
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| 张红霞等: "对苯二甲酸锂负极材料的溶剂热法合成", 《电源技术》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108766772A (en) * | 2018-04-23 | 2018-11-06 | 华东师范大学 | A kind of carbon coating titanium phosphate sodium and its preparation and application |
| CN108766772B (en) * | 2018-04-23 | 2019-11-15 | 华东师范大学 | A kind of carbon coating titanium phosphate sodium and its preparation and application |
| CN111525122A (en) * | 2020-05-12 | 2020-08-11 | 喻明兵 | NaTi2(PO4)3Negative electrode material of-porous carbon nanofiber sodium ion battery and preparation method thereof |
| CN111525122B (en) * | 2020-05-12 | 2021-07-27 | 苗珍录 | NaTi2(PO4)3Negative electrode material of-porous carbon nanofiber sodium ion battery and preparation method thereof |
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|---|---|
| CN106803582B (en) | 2019-06-14 |
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